HRID584221

反应详情

EQUATION

反应方程式

HRID 584221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl 2-acetylamino-2-(3,4-dimethylbenzyl)malonate (13.8 g) and potassium hydroxide (2.76 g) were dissolved into a mixed solution of ethanol (138 ml) and water (138 ml) and the solution was stirred under reflux for 8.5 hours. After being cooled to room temperature, the solution was concentrated under reduced pressure and the resulting aqueous solution was adjusted to pH 10 with aqeuous saturated sodium hydrogen carbonate solution. The solution was washed with ethyl acetate and made acidic with diluted hydrochloric acid, and extracted with ethyl acetate. The extract was dried over magnesium sulfate and evaporated under reduced pressure to give crystals of N-acetyl-3,4-dimethyl-DL-phenylalanine (5.42 g).

WORKUP

后处理

  1. temperatureunder reflux for 8.5 hours
  2. concentrationthe solution was concentrated under reduced pressure
  3. washThe solution was washed with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried over magnesium sulfate
  6. customevaporated under reduced pressure